CZ85397A3 - Oral preparation - Google Patents

Abstract

The invention relates to oral care products such as toothpastes with an improved sensorially-perceivable cleaning benefit. This is achieved by the inclusion in the oral care products of agglomerates, substantially free from organic and/or inorganic binding agents, whereby the agglomerates are made of at least two chemically and/or physically different particulate materials of specified particles sizes. The inclusion of materials having a therapeutic benefit on the teeth or gums in the agglomerates such as zinc citrate provides for a further benefit in that this material is slowly released from the agglomerates, thus providing for a delivery of this material over a longer period. Upon use, the gritty-feeling agglomerates will break-down into smaller particles, thus giving the consumer the feeling of initial cleaning and subsequent polishing.

Description

The present invention relates to oral compositions for use in the human mouth. More specifically, it relates to oral compositions comprising agglomerates of particulate materials, and these agglomerates provide oral compositions with a sensory, sensory benefit that is noticeable during the use of these oral compositions.

In particular, the present invention relates to oral compositions comprising an agglomerated particulate material comprising at least a particulate dental abrasive cleansing agent imparting a sensory perceptible cleaning benefit to the oral composition.

Prior art

Oral compositions of the above type have been proposed in the art. EP-A-269 966, EP-A-473 171 and GB-A-2 252 042 describe oral compositions comprising granules formed from particulate dental abrasive cleaning agents which have been agglomerated with organic or inorganic binders. During the use of such oral compositions in the mouth, the consumer perceives the presence of these granules, which gives him a sensory perception of the cleaning effect. During brushing of the teeth with these oral compositions, the granules are then comminuted by brush pressure to disintegrate into smaller particles, providing a polishing, smoothing effect that the consumer senses as a feeling of softness in both the oral composition and the teeth. Typical examples of such granules are formed from zeolite and colloidal silicon, using magnesium metasilicates or ethylcellulose as a binder.

GB-A-2 272 640 describes orally

- 2 devices with abrasive particles that are friable under the conditions in which the devices are used. These particles are formed from a particulate dental abrasive cleaning agent such as silica, agglomerated with water and subsequent drying in the absence of an inorganic or organic water-insoluble binder.

Although these earlier proposals may lead to oral means capable of providing some sensory benefit, this benefit is not very clear in some respects. Addition. if mixtures of different materials are agglomerated, this requires the use of an organic or inorganic binder, which makes the production of such agglomerates more costly.

The essence of the invention

The present inventors have now found that agglomerates, substantially free of organic and / or inorganic binders and having:

A) a particle size such that a D ₁₀ value equal to or greater than 50 micrometers, an O ₉₀ value equal to or less than 2000 micrometers, and a D _{50 value} ranging from 80 micrometers to 1500 micrometers, said agglomerates being formed of at least two particulate matter; materials and these materials differ chemically and / or physically from each other so that the at least one particulate material has

B) a particle size such that the D ₁₀ value is equal to or greater than 0.1 micrometer and the D _go value is equal to or less than 80 micrometers, the D ₅₀ value being in the range of 4 micrometers to 35 micrometers, and

C) the at least one further particulate material has a particle size such that the D ₁₀ value is equal to or greater than 0.1 micrometer and the D ₉₀ value is equal to or less than 100 micrometers, the D ₅₀ value ranging from 9 micrometers to 70 micrometers ,

- 3 provide, when incorporated into an oral composition, an oral composition which provides the consumer with a sensory perceptible cleansing and smoothing effect during the use of such an oral dentifrice.

The value of D ₁₀ is the particle size, based on a maximum of 10% by weight of the total amount of particles; thus, a D ₁₀ value of 50 micrometers means, for example, that no more than 10 weight percent of the total particles may have a particle size of 50 micrometers or less. The value of D ₅₀ indicates the particle size, where 50% by weight of the total amount of particles exceeds the stated value and 50% by weight of the total amount of particles is smaller than the stated value.

The value of D ₉₀ is the particle size at which 90% by weight of the total amount of particles should be equal to or less than this value.

For D ₁₀ , D _so and D ₉₀ according to A), the preferred values are:

D _w > 100 μm, especially> 150 μιτι D _go <1500 μm, especially <1000 μm

D ₅₀ from 150 [mu] m to 800 [mu] m, in particular from 200 [mu] m to 600 [mu] m.

For B) the following values are:

D ₁₀ > 2 μm, especially> 2.5 μm D ₉₀ <65 μm. in particular <40 μm D _with from 6 μm to 20 μm.

For C) the following values are:

D ₁₀ > 3 μm, especially> 4 μm

- 4 D _9θ <80 μΓη, especially <50 μιτι

D _5o from 10 μm to 40 μιτι.

All of the above particle sizes are measured using a Massage Model X instrument with an MG15 sample loading unit and using the measurement method outlined in the instruction manual and 300 micrometer lenses in the detector system.

A more accurate measurement of the actual agglomerate size distribution is obtained using network analysis.

100 g of the sample are placed on the top sieve from a series of BS sieves, consisting of sieves with a density graduating approximately 50 micrometres in the range of 45 to 600 micrometres. The sieves are arranged from the finest at the bottom to the coarsest top of the whole assembly. The screens are placed in a mechanical vibrator, such as the Inclyno Mechanical Sieve Shaker from Pascall Engineering Co. Ltd., closed with a lid and shaken for 10 minutes.

Each portion of a particular sieve is accurately weighed and the results are calculated according to the relationship:

weight of residue x 100% of residue = - ¹ weight of sample

The particle size distribution can then be evaluated from the data obtained.

The amount of chemically and / or physically different particulate materials in the agglomerates can vary from 70 to 100% by weight of the agglomerates and the equilibrium state, if any, is reached by other additives which will be discussed below. Relative weight ratio

- 5 chemically and / or physically different particulate materials in the agglomerate may vary from a ratio of 20:80 to a ratio of 80:20, preferably from a ratio of 25:75 to a ratio of 75:25.

The agglomerate-forming particulate materials are chemically and / or physically different from each other. Suitable particulate materials include particulate abrasive cleaners such as silicas, aluminas, calcium carbonates, calcium phosphates, calcium diphosphates, hydroxyapatites, perites. zeolites, pumice, volcanic ash, hectorites, saponites, aragonites, dolomites, magnesia, hydroxymagnesia, spangolites, zinc (zinc oxides), zinc silicates, meaphosphates and mixtures of two or more of the above materials. Examples of mixtures of particulate materials are silicon oxides with calcium carbonates, silicon oxides with calcium phosphate, silicon oxides with perlite, abrasive silicon oxides with thickening silicon oxides, hydroxyapatites with silicon oxides or meaphosphates, calcium carbonates with calcium phosphates, etc. gives mixtures of abrasive silicon oxides and thickening silicon oxides.

In addition, the authors have found that the inclusion of substances having a therapeutic effect on the gums or teeth or on the oral cavity in such agglomerates provides the additional advantage that during disintegration or disintegration of the agglomerate the therapeutic agent is slowly released and provides the therapeutic effect of the agent over time. section. Suitable examples of such therapeutic agents are zinc salts such as zinc citrate: antimicrobial agents such as Triclosan; anti-caries agents such as sodium fluoride and sodium monofluorophosphate; anti-plaque agents such as tin pyrophosphate; anti-tartar agents such as sodium pyrophosphate and potassium pyrophosphate; anti-sensitizing agents for the teeth such as potassium or strontium salts and the like.

In this respect, it has surprisingly been found that the incorporation of zinc citrate into agglomerates (up to 25% and preferably up to 12% by weight of agglomerates) has significantly reduced the level of astringent (perceived) ability perceived by experienced evaluators when testing toothpastes containing such agglomerates. on their sensory properties.

The invention will now be described in detail.

If the oral composition of the invention, such as toothpaste, is used in the mouth to clean teeth, the shear and / or disintegration forces generated should be sufficient to cause the agglomerate particles to disintegrate for some time. preferably in a short time in order to eliminate the sandy feeling felt by the user.

This means that the agglomerates should have a core strength such that they disintegrate in the range of shear and / or crushing forces normally generated with an appropriate tooth cleaning regime, as the considerable variable forces generated at individual locations over time allow at least some of the agglomerates survive unchanged long enough to perform their cleaning function to a satisfactory degree.

It is even possible to adjust the disintegration time of the agglomerates, for example by controlling the contact time at a given cleaning length of the composition, by controlling the average strength of the disintegration (crushing) of the agglomerates; for example, by selecting a particular type of source of particulate materials and / or the manner in which agglomeration is performed in the manufacturing process.

Upon disintegration of the agglomerates by shear forces and / or disintegration forces (crushing), the resulting average particle size (diameter) will typically be less than 60 micrometers. Such reduced particle sizes will generally be free from any perception of sandiness (crunchiness) in the mouth and

- 7 provide a feeling of smoothed (polished) teeth.

Particular preference is given to abrasive silicon oxides, such as low-structured silicon oxides, available from Crosfield Chemicals under the tradename AC77. Mixtures of different abrasive particulate materials can also be used.

The particulate thickeners (fillers) that can be used in the agglomerates can be any suitable particulate fillers, such as clays, but silicon oxide fillers (silicas) are preferred, for example filler silicas sold under the tradename Sident 22S (from Degussa). Other suitable silicon oxides include, for example, Zeodent 165 (from Zeofinn), Sorbosia TC 15 (from Crosfield Chemicals), Tixosil 43 (from Rhone-Poulenc) and Sylox 15X (from W. R. Grace).

Due to the porous structure of the agglomerates, they can act as transfer media for various substances such as color pigments, opacifiers, flavors, perfumes or other cosmetics, or, as already mentioned, for dental and / or oral therapeutic compounds. , for example fluoride compounds, for antibacterial agents such as Triclosan and zinc salts such as zinc citrate, for anti-caries compounds, for anti-calculus agents, for anti-hypersensitivity agents and the like. Such substances may be present in the pores of the material (e.g., after introduction into the pores by conventional techniques) and may, as particles disintegrating during use of the composition, be released from the composition when used in the mouth, for example, when brushing teeth.

A suitable industrial process for forming agglomerates, as described above, includes: spray-drying mixtures of particulate materials moistened with a suitable amount of a vaporizable liquid, such as water; granulation of a similar type to that used in the preparation of solids

- 8 detergents in granular form and pressure compression (compaction). Such procedures are well known in the art.

In the oral compositions of the present invention, the amount of agglomerates can vary widely, depending, for example, on the physical form of the desired product.

The compositions of the invention may be solids, in a form similar to, for example, conventional toothpastes or pastes, creams or gels, such as conventional toothpastes; or even fluids

Particularly preferred compositions of the invention are in the form of pastes, gels, creams or liquids, the exact physical properties of which can be controlled, for example, by appropriate adjustment of solid to liquid ratio and / or liquid phase viscosity, for example by selecting appropriate excipient contents, as described below.

In particularly preferred compositions of the invention, the agglomerates should be insoluble in the medium (medium) of the composition in which they are incorporated. In this context, the term insoluble indicates sufficient insolubility at ambient temperature so that the agglomerates remain insoluble or substantially insoluble in the composition, and therefore their friability under the conditions in which the composition is used and thus their ability to exhibit cleaning / polishing effect is not adversely affected. The insolubility of the agglomerates preferably extends to their insolubility in the oral environment in which the composition is used, which may often contain higher amounts of water than, for example, toothpaste, due to the presence of saliva and added water often used in brushing teeth.

In a preferred embodiment of the invention, the agglomerates are present in the compositions in amounts of from about 1 to 99 wt. %, better

- 9 from about 2 to 60 wt. % and more preferably from about 3 to 40% by weight. For liquid compositions, the last of the preferred intervals is particularly suitable. In the compositions according to the invention in the form of a paste, the agglomerates are preferably present in an amount of approximately from 1 to 25 wt. %, more preferably from about 1 to 15 wt. % and more preferably from about 2 to 10% by weight.

The oral compositions of the invention may contain one or more additional ingredients, as will now be described.

The oral compositions of the invention preferably comprise one or more surfactants, preferably selected from anionic, nonionic. amphoteric and zwitterionic surfactants and mixtures thereof, all of a nature suitable for dental and / or oral use.

Suitable anionic surfactants may include soaps, alkyl sulfates, alkyl ether sulfates, alkaryl sulfonates, alkanoyl isethionates, alkanoyl taurates, alkyl succinates, alkyl sulfosuccinates, N-alkoxyl sarcosinates, alkyl phosphates, alkyl ether phosphates, alkyl ether carboxylates, especially sodium halocarboxylates, and alpha-salts. di- and triethanolamine salts. Alkyl and acyl groups generally contain 8 to 18 carbon atoms and may be unsaturated. Alkyl ether sulfates, alkyl ether phosphates and alkyl ether carboxylates may contain from 1 to 10 ethylene oxide or propylene oxide units per molecule and preferably contain 2 to 3 ethylene oxide units per molecule.

Examples of preferred anionic surfactants may include sodium lauryl sulfate, sodium dodecylbenzenesulfonate, sodium lauroyl sarcosinate, and coconut monoglyceride sulfonate.

Nonionic surfactants that may be suitable for

Uses in the compositions of the invention include sorbitan and polyglycerol fatty acid esters, as well as block copolymers of ethylene oxide and propylene oxide.

Amphoteric surfactants that may be suitable for use in the compositions of the invention include, for example, betaines. such as coconut amidopropyl betaine, and sulfobetaines.

The surfactant or substances may be present in the oral composition of the invention in a total amount of from about 0.1 to 3% by weight.

Another preferred component of the oral compositions of the invention is water, which may be present in an amount of from about 1 to 90% by weight, more preferably from about 10 to 60% by weight. % and most preferably from about 15 to 50% by weight.

The toothpastes and creams of the present invention may also contain moisturizing agents, for example, polyols such as glycerol, sorbitol syrup, polyethylene glycol, lactitol, xylitol, and hydrogenated corn syrup. The total amount of wetting agent, if present, may range, for example, from about 10 to 85% by weight of the composition.

In the oral compositions of the present invention, it is particularly preferred to incorporate one or more thickening agents and / or suspending agents to provide the composition with the desired physical properties (e.g., paste, cream or liquid) and to ensure that the agglomerates remain in stably dispersed in the composition.

Particular preference is given to concentrating oral compositions according to

The present invention provides for the inclusion of conventional thickening agents, such as silica thickeners, silica, examples of which have been exemplified above.

Other suitable suspending / thickening agents are well known in the art and include, for example, polyacrylic acid, copolymers and crosslinked polymers of acrylic acid, copolymers of acrylic acid with hydrophobic monomer, copolymers of carboxylic acid-acrylic ester monomer, crosslinked copolymers of acrylic acid and acrylate esters, esters ethylene glycol or polyethylene glycol esters (e.g. fatty acid esters thereof), heteropolysaccharide gums and cellulose derivatives such as sodium carboxymethylcellulose.

Particularly suitable thickening agents are heteropolysaccharide gums such as xanthan gum and guar gum.

The thickening agent and / or suspending agent (which may be used alone or as a mixture of two or more such materials) may be present in the composition in a total amount of from about 0.1 to about 50% by weight; preferably from about 5 to 15% for silica thickeners and preferably from about 0.1 to 5% for polymeric suspending agents.

The compositions of the invention may contain one or more other ingredients commonly found in oral compositions. Suitable additional ingredients include: flavors, eg menthol, peppermint; artificial sweeteners; perfumes or breath fresheners; pearlescent agents, peroxy compounds, for example hydrogen peroxide or peracetic acid, opacifying agents; dyes and coloring agents; preservatives; wetting agents, fluoride-containing compounds; anti-caries agents; anti-plaque agents; therapeutic agents such as zinc citrate, Triclosan (from

- 12 Ciba-Geigy); proteins; salts and pH adjusting agents. In addition, the compositions usually contain additional abrasive cleaning agents in an amount of 5 to 60% by weight, such as abrasive silicas, chalks, hydrated aluminas, calcium phosphate, calcium pyrophosphates, hydroxyapatites, insoluble metaphosphates and the like.

The compositions of the present invention may be manufactured by conventional methods of manufacturing oral compositions. Pastes and creams can be made by conventional methods, for example, using high shear mixing systems under vacuum, and by adding agglomerates characterizing the invention to the premixed base composition only in a second step, which involves dispersing / mixing in the preformed composition under low shear conditions. shear (small shear forces).

In the manufacture of the compositions of the invention, this is generally important. that any mixing step carried out is carried out at a sufficiently low shear and / or speed so that the agglomerates according to the invention do not come into contact with forces so great as to cause the particles to break.

The oral compositions of the invention may be used in a manner similar to conventional oral compositions, e.g. toothpastes, i.e. a suitable amount of the composition is applied to a toothbrush or directly to the mouth and, if necessary with the addition of a certain amount of water, and a slurry acts on the teeth, gums and / or, if necessary or desired, on other parts of the mouth so that the effects of the agglomerates are applied to the intended surfaces in the mouth. Due to the friability of the agglomerates, any perception of sandiness felt by the user will soon be lost; so that once the agglomerates have demonstrated their cleaning function, the composition is free to exert another polishing effect or, for example, to exert one or more other beneficial functions provided by the other components of the composition. Finally, the mouth can be rinsed with water, as with normal oral products. This procedure can be used

- 13 repeated as many times as desired.

The invention is further illustrated by the following examples.

Examples of embodiments of the invention

Example 1

The following particulate (loose) silicas were mixed together and blended with zinc citrate and / or titanium dioxide trihydrate to provide a perfect mixture:

and 1 parts by weight 2 parts by weight Sorbosil AC 77 (*) 43.15 48.5 Sorbosil TC15 (*) 43.15 48.5 titanium dioxide 3.0 3.0 zinc citrate trihydrate 10.7 0.0

Silicas had the following properties:

Sorbosil AC77 Sorbosil TC15 surface area (m ² / g) 120 260 diameter D, _o 2.7 5.6 diameter 8.1 12.9 diameter D _m 17.8 29.3

(*) available from Joseph Crosfield & Sons, England

Water was added to this mixture to obtain a water to solids ratio of 1.33: 1, and the resulting mixture was granulated in a pan granulator.

The resulting wet agglomerates were then dried in an oven at room temperature for 4 hours

- 14 120 ° C, or partially dried in 30 minutes in a fluid bed dryer and dried in an oven at the same temperature as in the first case for 2 hours. The particle size distribution was adjusted by sieving at 150 and 400 micrometers.

The weight average particle size of the silica and agglomerates was determined using a Malvem Mastersizer Model X instrument with an MS15 ”sample delivery unit. Prior to the measurement described in the instrument's instruction manual and using 300 micrometer lenses in the detector system, the silica were scattered by ultrasound and the agglomerates were mixed mechanically.

After determining the weight average particle size distribution of the agglomerates as described above, another sample of agomerates was dispersed using ultrasonic disintegration for 2 minutes and set to 100. It was then subjected to a measurement procedure. Thus, the values of D ₁₀ , D ₅₀ and D _w can be derived (interpolated) from the particle size distribution, and the higher the values obtained after subjecting the sample to ultrasonic disintegration, the stronger the agglomerates.

The following results were obtained:

disintegration ultrasound D ₁₀ Dso Dgo mixture 1 0 193 334 502 100 3.3 14.3 42 mixture 2 0 268 391 539 100 3.3 12 39

A toothpaste of the following composition was prepared with the agglomerates of mixture 1:

ADDITIVES% w / w) sorbitol syrup 70%

45.00

sodium fluoride 0.32 saccharin 0.20 titanium dioxide 0.10 polyethylene glycol (mol. wt. 1500) 5.0 blue No. 1 0.0003 Abrasive silica (AC77) 8.0 thickening silica (TC15) 7.0 cellulose rubber (CMC9) 0.80 sodium lauryl sulfate 1.80 flavor 1.20 agglomerates of a mixture 1 7.0 water up to 100

This preparation (A) was subjected to a qualitative descriptive analysis test using experienced evaluators, comparing the preparation with preparation (B) containing zeolite agglomerates according to EP 269 966 in a comparison test.

The following results were obtained (using a scale of 0-10);

visibility factor hardness ease of upset preparation A 5.5 3.7 7.7 preparation B 6.0 _; _ 4.0 7.0

When the ratio of TC15 and AC77 in the agglomerates of mixture 1 was changed to 75:25 (C), the following data were obtained:

visibility factor hardness ease of upset preparation C 4.1 4.2 6.8 ί

- 16 Example 2

Repeating Example 1, but using agglomerates of mixture 2, gave the following results:

visibility factor hardness ease of upset preparation A ¹ 7.1 6.5 5.1 preparation B ' 6.0 4.0 7.0

When the ratio of TC15 and AC77 in the agglomerates of mixture 2 was changed to 75:25 (D), the following data were obtained:

visibility factor hardness ease of upset preparation D 4.1 5.1 6.4

Example 3

The agglomerates of mixture 1 were tested for their ability to retain zinc citrate. The agglomerates were ground in water to a slurry (Example 1) and in a sorbitol / water mixture (Example 2) and the amount of zinc ions released into the water or into the sorbitol / water mixture was determined at different time intervals. The following results were obtained:

% solubility of Zn time (mm.) 60 480 1440 2880 Example 1 36.57 35.45 36.29 34.94 Example 2 12.24 12.25 13.47 13.29

Zinc release from agglomerates during cleaning was also measured using a cleaning device. It was found that after 2 minutes of cleaning, 60% of the available zinc was released using a smooth surface and 70% using a sandy (granular) surface.

- 17 Comparison of a commercially available toothpaste containing zinc citrate,

Mentadent P, with Formulation A, regarding the astringent action of the products, was performed using a qualitative descriptive analysis test performed by experienced evaluators. A value of 7.6 was obtained for Mentadent P and a value of 4.0 for Preparation A.

Example 5

Example 4

A number of different agglomerates were prepared and their sensory properties were tested in the toothpaste preparation A or B by three evaluators.

The toothpaste preparation A had the following composition:

ADDITIVES% (wt.)

sorbitol 70% 45.00 sodium fluoride 0.32 sachann 0.20 titanium dioxide 0.10 polyethylene glycol (mol. wt. 1500) 5.00 blue No. 1 0.0005 abrasive silica 8.00 thickening silica 7.00 carboxymethylcellulose (CMC9) 0.80 sodium lauryl sulfate 1.80 flavor 1.00 agglomerates 7.00 water up to 100

The toothpaste preparation B had the following composition:

INGREDIENTS % (wt.) glycerol 35.00 sodium fluoride 0.32 saccharin 0.27 titanium dioxide 1.00 polyethylene glycol (mol. wt. 1500) 5.00 abrasive silica 8.00 thickening silica 7.00 sodium bicarbonate 10.00 carboxymethylcellulose (CMC9) 0.70 sodium lauryl sulfate 1.80 flavor 1.50 agglomerates 7.00 water up to 100

All agglomerates exhibited a particle size distribution ranging from 150 to 400 micrometers, and all of the particulate material from which the agglomerates were formed exhibited a particle size distribution in the ranges set forth in this application.

The agglomerates had the following composition:

weight%

AND

and and λ— 57 F 1 1 and ι 1 1 and and 1 ί ¹ I o i ro v- CO ; and o r- T-: CD 1 ¹ I '' t 1 1 t 1 co ¹ co 1 CT) o o X ^{- 1} 1 1 1 ι i; . what 1 45 1 1 1 LO IN 2 '' i 1 and 1 . O- 50 1 1 t 1 O LO ^{11 1} 1 ^! <0 1! LO T 1 and 1 1 1 and LO 45 1 22.5 LO oj ' 04 1 1 10 T ! 45 45 1 1 1 1 and O T- ' and I WHAT 50 1 1 1 50 1 I 1 : i ι i 1 CN 1 50 1 LO OJ LO OJ 1 t 1 1. 1 1 50 50 1 1 1 1 and 1 1 1 t and 1 natý

-> s + · *

CD

C

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4— * I iz ra c

ra

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and- and 1 and 22 J O WHAT LO Lf) ; r- 30 ! - o, and ι 1 what O- 0- 1 and 1 what 1 I 04 what IN" WHAT 1 1 O ¹ 1 LO 1 O ιθ OJ 1 O 1 and σ> and 1 ! O O LO LO 1 and 1 WHAT LO LO O 1 1 1 1 Xt | i | and O- h- what and CD WHAT! and <O OJ OJ WHAT O and OJ OJ T r- LO LO LO O OJ OJ LO ¹ 1! tn Lf) LO sS ¹ OJ Ol 1 O Ol OJ C - * - · ω O what O O T- LO 1 LO 1 O E _ £ Z 04 1 CD LO Lf LO 04 OJ 1 ! 1 ·> .; ra -> X C O ra ra no ·> ra foam ra apene IX -ra > C C 'CD ra > ra ra CL 'CD > > C ra ací s silicon C ra ra CZ C > o CD l_ C > ‘- > O G) Oh ^! C Ό CZ ie M—! ra ra > -C N (Λ > ω □ O > o £ 3 SW <u C ώ <5 M— O to. SW ra JD Φ >. * - * > x 3 N ra Cl zr θ CL

- 20 The results of the sensory properties tests were as follows.

agglomerate Toothpaste particle perception sensation in the mouth during use -------— J 1 B very good good 2 B good good ^! 3 B difficult good 4 B very good good i 5 B good good 6 B difficult good _ 7 B difficult good 8 B very good good 9 B very good good; 10 AND very good good 11 AND difficult good 12 AND very good good 13 AND very good sandy, 14 AND very good slightly sandy 15 B very good good 16 . B very good good 17 AND very good sandy 18 AND very good sandy! 19 AND very good sandy; 20 AND very good good ²¹ AND very good gritty 22 AND very good sandy j

The agglomerates described below, prepared by dry compression, have also been tested in toothpaste formulation A and can be perceived very well, with good mouthfeel. The agglomerates had a particle size distribution between 150 and 400 micrometers and the particulate material from which the agglomerates were formed showed a particle size distribution in the ranges given in this application.

- 21 Agiomerates had the following composition:

weight%

number 1 2 3 4 5 6; 7 8 abrasive silica _ 10.3 23.81 26.3 23.3 27.65 24.5 36 41 thickening silica 10.3 23.81 26.3: 23.3 27.65 24.5 I 36 41 titanium dioxide 3.0 3.0 3.0 3.0 3.0 3.9 to 3.0 3.0 potassium 76.4 43.3 - ! - potassium pyrophosphate 24.6 24.6 - and tetrasodium pyrophosphate 19.8 ^: 19.8 - potassium nitrate - - - 41.7 41.7 ^: - stannous pyrophosphate - - - - j 14.29 Triclosan - - - - 4.3

Represents:

Claims (10)

An oral composition comprising agglomerates of particulate material, characterized in that said agglomerates are substantially free of organic and / or inorganic binders and said agglomerates have A) a particle size such that a D ₁₀ value is equal to or greater than 50 microns; value D _w is equal to 2000 microns or less, and D ₅₀ in the range from 80 micrometers to 1500 micrometers, wherein said agglomerates are formed from at least two particulate materials, and these materials are chemically and / or physically different, so that at least one the particulate material had B) a particle size such that the D ₁₀ value is equal to or greater than 0.1 micrometer, the D _M value is equal to or less than 80 micrometers and the D ₅₀ value is between 4 micrometers and 35 micrometers, and C) at least one other particulate material has a particle size such that a D ₁₀ value is equal to or greater than 0.1 micrometer and equal to or less than 100 microns, with a D _{50 of} from 9 microns to 70 microns. Oral composition according to claim 1, characterized in that for A) D is ₁₀ > 100 µm, <1500 µm and D _{M is} from 150 µm to 800 µm, for B) D is ₁₀ > 2 µm, Dgg <65 µm and D ₅₀ from 6 µm to 20 µm, and for C) D is ₁₀ > 3 µm, D _w <80 µm and from 10 µm to 40 µm. Oral preparation according to claim 2, characterized in that for A) D _{10 is} > 150 pm, D ₉₀ <1000 pm and D _{s is} from 200 pm to 600 pm, for B) D _{10 is} > 2.5 pm, D ₃₀ <40 pm and for C) D ₁₀ > 4 pm and D ₉₀ <50 pm. 4. An oral formulation according to claim 1, 2 or 3 wherein the agglomerates comprise at least 70% by weight of particulate materials. The oral composition of claims 1 to 4, wherein the agglomerates further comprise a substance having a cosmetic or therapeutic dental effect. - 23 The oral composition of claim 5, wherein the agglomerates comprise a zinc compound. Oral composition according to claims 1 to 6, characterized in that it contains agglomerates in an amount of 1 to 99% by weight. Oral composition according to claim 7, characterized in that it contains agglomerates in an amount of 3 to 40% by weight. Oral composition according to claims 1 to 8, characterized in that the agglomerates are formed from a mixture of thickening and abrasive silicas in a relative weight ratio of from 75:25 to 25:75. The oral composition of claim 9, wherein the agglomerates comprise thickening and abrasive silicas in a relative weight ratio of 50:50 and further comprise titanium dioxide and zinc citrate.